CN101885583A - Method for preparing erbium-containing red glass - Google Patents
Method for preparing erbium-containing red glass Download PDFInfo
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- CN101885583A CN101885583A CN 201010198343 CN201010198343A CN101885583A CN 101885583 A CN101885583 A CN 101885583A CN 201010198343 CN201010198343 CN 201010198343 CN 201010198343 A CN201010198343 A CN 201010198343A CN 101885583 A CN101885583 A CN 101885583A
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Abstract
The invention relates to a method for preparing erbium-containing red glass, which comprises the following steps of: firstly, mixing P2O5, BaO, Al2O3, Er2O3, CeO2 and Fe2O3 uniformly, and then melting the mixture to obtain glass liquid; secondly, performing water quenching on the glass liquid, and then drying and performing ball milling to be 50 meshes to obtain coloring agent glass; thirdly, after mixing P2O5, BaO, Al2O3, Fe2O3 and the coloring agent glass uniformly, melting the mixture; pouring the bubble-free molten glass liquid into a metal mould for molding; fourthly, placing the molded glass sample into a muffle furnace at the temperature of 450 DEG C for 3 hours, raising the temperature to be 600 DEG C at the speed of 20 DEG C per minute and preserving the heat for 1 hour; and finally, cooling the glass sample to room temperature at the speed of between 0.5 and 1 DEG C per minute to obtain the erbium-containing red glass. The erbium-containing red glass is prepared by a high temperature melting method; the method has the advantages of simple operation procedure, low melting temperature, low cost, energy conservation, environmental protection and suitability for industrial production; and the erbium-containing red glass prepared by the method has the advantages of high chemical stability, uniform coloring, high light transmittance and stable product quality.
Description
Technical field
The present invention relates to a kind of preparation method of red glass, particularly a kind of preparation method of erbium-containing red glass.
Background technology
Along with the raising of people's living standard, coloured glass more and more is subjected to people's attention.Red glass especially is subjected to human consumer's favor with its bright colour.The red glass that can prepare by the high temperature melting method has: the antimony ruby glass of the neodymium red glass of the selenium cadmium red glass of large red, bolarious copper ruby glass, gold ruby glass rosy, violet redness, peach erbium red glass, cherry-red.Up to the present, the production technology of selenium cadmium red glass is the most ripe, produces the most stable, most widely used general.Though selenium cadmium red glass color is beautiful, but owing to contain cadmium in the glass, electrical equipment and electronics offal treatment method (Waste Electnical and Electronic Equipment according to EU countries's promulgation, WEEE), banned use of the material that contains Pb, Cd, Hg, Tl in 2008.China classified as the heavily contaminated element such as lead, cadmium, mercury and bismuth on January 1st, 2006.Therefore, selenium cadmium red glass in use is restricted.Generally, when containing the rare metal erbium in the glass, the color of glass is a pink, and its color selenium cadmium crimson glass that is far from is bright-coloured like that.Do not appear in the newspapers about the large red glass that contains erbium.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of fill a prescription form less, the preparation method of the simple erbium-containing red glass of technological process, the large red glassy product steady quality that obtains according to preparation method of the present invention, the uniform coloring of glass, and preparation technology's operating process is simple, with low cost, be suitable for suitability for industrialized production.
For achieving the above object, the technical solution used in the present invention is: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 40～70% P
2O
5, 20～40% BaO, 1～5% Al
2O
3, 1～30% Er
2O
3, 0.1～5% CeO
2With 0.0001～0.01% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1300～1350 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 40～70%P
2O
5, 20～40%BaO, 1～5%Al
2O
3, 0.0001～0.01%Fe
2O
3, 5～20% above-mentioned colouring agent glass mix; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 1～4 hour at 1300～1350 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 0.5～1 ℃/minute speed and namely get the large red glass that contains erbium.
Said P
2O
5Introduced by analytically pure ammonium dihydrogen phosphate (ADP); Said BaO is introduced by analytically pure brium carbonate; Said Al
2O
3Introduced by analytically pure aluminium hydroxide; Said Er
2O
3Introduced by analytically pure erbium oxide; Said CeO
2Introduced by analytically pure cerium oxide; Said Fe
2O
3Introduced by analytically pure iron oxide.
The present invention prepares the large red glass that contains erbium by high-temperature melting method, and preparation technology's operating process is simple, and glass melting temperature is low, and is with low cost, and energy-conserving and environment-protective are suitable for suitability for industrialized production.The erbium large red glass chemistry that contains that obtains according to preparation method of the present invention has good stability uniform coloring, transmittance height, constant product quality.
Description of drawings
Fig. 1 is the sample light transmittance curve figure that contains erbium large red glass of embodiment 1 preparation, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Fig. 2 is the sample light transmittance curve figure that contains erbium large red glass of embodiment 2 preparations, and wherein X-coordinate is a lambda1-wavelength, and ordinate zou is a transmittance.
Embodiment
Embodiment 1: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 60% P
2O
5, 27% BaO, 3.5% Al
2O
3, 7% Er
2O
3, 2.49% CeO
2With 0.01% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1300 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 61%P
2O
5, 30%BaO, 3.99%Al
2O
3, 0.01%Fe
2O
3, 5% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 2 hours at 1350 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 1 ℃/minute speed and namely get the large red glass that contains erbium.
The density of measuring sample by Archimedes's method is 3.26g/cm
3, the light transmittance curve by the spectrophotometer test sample as shown in Figure 1.
Embodiment 2: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 57% P
2O
5, 30% BaO, 3.5% Al
2O
3, 7% Er
2O
3, 2.49% CeO
2With 0.01% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1300 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 55%P
2O
5, 33%BaO, 3.99%Al
2O
3, 0.01%Fe
2O
3, 8% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 4 hours at 1350 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 0.5 ℃/minute speed and namely get the large red glass that contains erbium.
The density of measuring sample by Archimedes's method is 3.29g/cm
3, shown in Figure 2 by the light transmittance curve of spectrophotometer test sample.
Embodiment 3: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 40% P
2O
5, 25% BaO, 1% Al
2O
3, 30% Er
2O
3, 3.9999% CeO
2With 0.0001% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1350 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 70%P
2O
5, 20%BaO, 1%Al
2O
3, 0.0001%Fe
2O
3, 8.9999% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 4 hours at 1300 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 0.8 ℃/minute speed and namely get the large red glass that contains erbium.
Embodiment 4: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 70% P
2O
5, 20% BaO, 5% Al
2O
3, 1% Er
2O
3, 3.995% CeO
2With 0.005% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1320 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 40%P
2O
5, 40%BaO, 5%Al
2O
3, 0.03%Fe
2O
3, 14.97% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 2 hours at 1340 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 0.5 ℃/minute speed and namely get the large red glass that contains erbium.
Embodiment 5: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 50% P
2O
5, 40% BaO, 1.899% Al
2O
3, 8% Er
2O
3, 0.1% CeO
2With 0.001% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1340 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 50%P
2O
5, 25%BaO, 4.995%Al
2O
3, 0.005%Fe
2O
3, 20% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 3 hours at 1320 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 1 ℃/minute speed and namely get the large red glass that contains erbium.
Embodiment 6: the first step: the preparation 1 of colouring agent glass) at first, and by mass percentage with 45% P
2O
5, 27% BaO, 2.95% Al
2O
3, 20% Er
2O
3, 5% CeO
2With 0.05% Fe
2O
3Mix; 2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1310 ℃, and is incubated 60 minutes under glass melting temperature; 3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass dregs of shrend is taken out, and oven dry ball milling to 50 order namely gets colouring agent glass; Second step: the preparation 1 of red glass) at first, by mass percentage with 50%P
2O
5, 35%BaO, 2.95%Al
2O
3, 0.05%Fe
2O
3, 12% above-mentioned colouring agent glass mixes; 2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, founds 1 hour at 1330 ℃ after crucible cover is covered; 3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; Then the glass specimen of moulding is put into 450 ℃ Muffle furnace insulation after 3 hours, be warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again; 4) last, be cooled to room temperature with 1 ℃/minute speed and namely get the large red glass that contains erbium.
The present invention prepares the large red glass that contains erbium by high-temperature melting method, and preparation technology's operating process is simple, and glass melting temperature is low, and is with low cost, and energy-conserving and environment-protective are suitable for suitability for industrialized production.The erbium large red glass chemistry that contains that obtains according to preparation method of the present invention has good stability, uniform coloring, and the transmittance height, constant product quality can be used as the substitute products of selenium cadmium red glass.Therefore, have considerable economic and social benefit with the standby red glass of the party's legal system, application prospect is very wide.
Claims (3)
1. the preparation method of an erbium-containing red glass is characterized in that:
The first step: the preparation of tinting material glass
1) at first, by mass percentage with 40～70% P
2O
5, 20～40% BaO, 1～5% Al
2O
3, 1～30% Er
2O
3, 0.1～5% CeO
2With 0.0001～0.01% Fe
2O
3Mix;
2) secondly, add this raw material that mixes in the corundum crucible under 1100 ℃ or the bique crucible and be melted into glass metal, glass melting temperature is 1300～1350 ℃, and is incubated 60 minutes under glass melting temperature;
3) last, with the glass metal shrend in room temperature water that melts in the crucible, crucible is put back in the stove, and makes furnace temperature remain on 1100 ℃; The glass slag of shrend is taken out, and oven dry ball milling to 50 order promptly gets tinting material glass;
Second step: the preparation of red glass
1) at first, by mass percentage with 40～70%P
2O
5, 20～40%BaO, 1～5%Al
2O
3, 0.0001～0.01%Fe
2O
3Mix with 5～20% above-mentioned colouring agent glass;
2) secondly, it is in 1100 ℃ the corundum crucible or bique crucible that this raw material that mixes is added above-mentioned furnace temperature, crucible cover is covered the back founded 1～4 hour at 1300～1350 ℃;
3) will found complete bubble-free glass metal and pour moulding in the metal die that is preheated to 400 ℃ into; The retort furnace insulation of then glass specimen of moulding being put into 450 ℃ is after 3 hours, is warming up to 600 ℃ of insulations 1 hour with 20 ℃/minute speed again;
4) last, be cooled to room temperature with 0.5～1 ℃/minute speed and promptly get the large red glass that contains erbium.
2. the preparation method of erbium-containing red glass according to claim 1 is characterized in that: said P
2O
5Introduced by analytically pure ammonium dihydrogen phosphate (ADP); Said BaO is introduced by analytically pure brium carbonate; Said Al
2O
3Introduced by analytically pure aluminium hydroxide; Said Er
2O
3Introduced by analytically pure erbium oxide; Said CeO
2Introduced by analytically pure cerium oxide; Said Fe
2O
3Introduced by analytically pure iron oxide.
3. the preparation method of erbium-containing red glass according to claim 1 is characterized in that: used crucible is for having founded tinting material glass or having carried out crucible after erbium-containing red glass is founded.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101983435A CN101885583B (en) | 2010-06-11 | 2010-06-11 | Method for preparing erbium-containing red glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101983435A CN101885583B (en) | 2010-06-11 | 2010-06-11 | Method for preparing erbium-containing red glass |
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|---|---|
| CN101885583A true CN101885583A (en) | 2010-11-17 |
| CN101885583B CN101885583B (en) | 2012-01-25 |
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|---|---|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417951A (en) * | 2015-12-03 | 2016-03-23 | 李嘉 | Preparation method of high temperature resistant yellow glass |
| CN105439443A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant blue glass |
| CN105439442A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant black glass |
| CN105439447A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant purple glass |
| CN105439449A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant milk white glass |
| CN105439448A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant red glass |
| CN105439444A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant green glass |
| CN105481249A (en) * | 2015-12-03 | 2016-04-13 | 李嘉 | Preparation method of high temperature-resistant claret-colored glass |
| CN106116144A (en) * | 2016-08-04 | 2016-11-16 | 陕西科技大学 | A kind of preparation method of red high-boron-silicon glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417951A (en) * | 2015-12-03 | 2016-03-23 | 李嘉 | Preparation method of high temperature resistant yellow glass |
| CN105439443A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant blue glass |
| CN105439442A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant black glass |
| CN105439447A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant purple glass |
| CN105439449A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant milk white glass |
| CN105439448A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant red glass |
| CN105439444A (en) * | 2015-12-03 | 2016-03-30 | 李嘉 | Method for preparing high-temperature resistant green glass |
| CN105481249A (en) * | 2015-12-03 | 2016-04-13 | 李嘉 | Preparation method of high temperature-resistant claret-colored glass |
| CN106116144A (en) * | 2016-08-04 | 2016-11-16 | 陕西科技大学 | A kind of preparation method of red high-boron-silicon glass |
| CN106116144B (en) * | 2016-08-04 | 2018-06-15 | 陕西科技大学 | A kind of preparation method of red high-boron-silicon glass |
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|---|---|
| CN101885583B (en) | 2012-01-25 |
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